HRID2222041

反应详情

EQUATION

反应方程式

HRID 2222041 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of {4-({4-[({4-[(E)-2-(2-ethyl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy}methyl)-5-methyl-2-(3-nitrophenyl)-1,3-oxazole (650 mg), iron (reduced) (284 mg), calcium chloride (11 mg) and 80% ethanol (8 mL) was heated under reflux for 2 hrs. Insoluble materials were removed by celite filtration, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate to give {3-[4-({4-[({4-[(E)-2-(2-ethyl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy}methyl)-5-methyl-1,3-oxazol-2-yl]phenyl}amine as yellow amorphous form (150 mg, yield 38%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hrs
  3. customInsoluble materials were removed by celite filtration
  4. concentrationthe filtrate was concentrated
  5. washeluted with ethyl acetate